Fast Optically Stimulated Luminescence Component Research Articles

Tracing uplift and erosion in orogenic settings using quartz luminescence sensitivity: Insights from the Northern Andes uplift

The optically stimulated luminescence (OSL) sensitivity of the fast component in quartz has been increasingly used in provenance analysis of Quaternary sediments. Quartz OSL natural sensitization is thought to be mainly controlled by the formation conditions of the source bedrock and surface processes occurring mainly in sediment source areas. Thus, quartz OSL sensitivity can be linked to distinct sediment source regions, based on their tectonic setting and erosion conditions. In this way, changes in quartz OSL sensitivity within siliciclastic successions would track variations in sediment provenance. So far, few works evaluated how the OSL sensitivity of quartz sand grains varies in sedimentary successions that experienced long-term cycles of deep burial, exhumation, and erosion. Therefore, this work aims to characterize the sensitivity of the fast OSL component of quartz sand grains retrieved from the Cenozoic sedimentary rocks of the Northern Andes basins and assess its spatiotemporal changes. We found that quartz grains with the lowest OSL sensitivity are sourced by crystalline and volcanic rocks related to the Andean Continental Arc emplaced in the Colombian Central Cordillera, reflecting the onset of denudation in orogenic sources during the Paleocene. Subsequently, increasing trends in OSL sensitivity are related to the sedimentary recycling during the Andean orogeny, reaching maximum values as a result of the progressive unroofing of Cretaceous rocks in the Colombian Eastern Cordillera, originally sourced from the low-relief Amazon Craton. Changes in quartz OSL sensitivity measured in the Cenozoic sedimentary basin-fill sequences of the Northern Andes vary according to the shifts in sediment provenance related to the orogenic construction and sediment recycling of the Andean range.

Effect of alpha irradiation on the saturation characteristics of fine-grained quartz OSL

A negative relationship has been reported for the characteristic saturation dose (D0) of the quartz optically stimulated luminescence (OSL) signal and the quartz grain size, of which the mechanism is still not understood. Here, the natural coarse-grained quartz samples (63–90 μm, 90–125 μm) are artificially ground into fine grains and the effect of alpha irradiation on the D0 values of the ground fine grains is investigated. The ground fine grains (4–11, 11–45, 45–63 μm) have similar D0 values as the coarse grains. Laboratory alpha irradiation is administered on the artificial 4–11 μm quartz fraction. The D0 shows an increasing trend with the amount of alpha irradiation; meanwhile, the proportion of the fast OSL component decreases and the proportions of the medium and slow components increase with alpha irradiation. The higher D0 after alpha irradiation may be a result of the higher proportion of electron traps related to the medium component. However, the increasing trend of D0 stops when the alpha dose reaches a certain amount, and the degree of D0 increase induced by alpha irradiation cannot fully account for the much higher D0 values of the fine quartz grains in nature.

Trap Parameters for the Fast OSL Signal Component Obtained through Analytical Separation for Various Quartz Samples

Trap stability is essential in luminescence dating and thermochronometry. Trap depth and frequency factors determining the stability of the fast component of optically stimulated luminescence (OSL) in quartz, which is the most important in dating, have yet to be uniquely determined, especially for samples with an OSL signal not dominated by this component. One can determine them in OSL thermal depletion curve (OTDC) experiments. The separation of the fast OSL signal undisturbed by other OSL components is vital for obtaining accurate parameters for the traps of interest. This work presents a method of simultaneous thermal and optical stimulation using red light (620 nm) to separate the fast OSL component (the thermally modulated OSL method-TM-OSL). The OTDC experiment with the TM-OSL stimulation was used for the trap parameter determination on a variety of quartz samples, leading us to report for the first time, the trap parameters for the fast OSL component analytically separated in quartz from rock samples. The results obtained for these samples with the fast component of low intensity are consistent with those with an intensive fast OSL component. Results of OTDC measurements for all investigated quartz samples were tested for a wide range of irradiation doses.

Luminescence signals of quartz and feldspar as new methods for stratigraphic discrimination and provenance analysis of siliciclastic successions: The case of the Parnaíba Basin (Brazil) of West Gondwana

AbstractLuminescence characteristics of quartz and feldspar allow to discriminate sediments from different source areas. Particularly, sensitivity of optically stimulated luminescence (OSL) and thermoluminescence (TL) signals of quartz and infrared‐stimulated luminescence (IRSL) of feldspar from Quaternary sediments has been used for provenance analysis. These properties change due to source area denudation rates and sediment reworking, which drive the number of burial irradiation‐solar exposure cycles of sediment grains in surface systems. Here, we use for the first time a similar approach to interpret the geomorphic conditions of source areas of Silurian to Triassic siliciclastic sedimentary units of the intracratonic Parnaíba Basin in northeast Brazil. Luminescence measurements were performed on sand grains, and statistical tests were applied to evaluate differences in luminescence properties within and across stratigraphic units. We explored the position of well‐known “110°C” (TL110) and “325°C” (TL325) TL peaks of quartz as proxies to discriminate stratigraphic units with similar lithological assemblages. OSL and TL sensitivities as well as the dominance of the so‐called fast OSL component increase from Silurian to Triassic sedimentary units, while the IRSL sensitivity decreases towards younger stratigraphic units. These patterns point to source areas with decreasing denudation rate and higher sediment recycling over basin filling time, leading to decreasing feldspar concentration and quartz luminescence sensitisation. Major changes in luminescence properties coincide with regional unconformities. This is attributed to physical landscape changes leading to shifts in the relief of source areas and basin sediment recycling. The TL110peak position is similar across stratigraphic units, but the TL325peak position has significant variation, with values between 324°C and 334°C, allowing its use for stratigraphic discrimination. Changes in OSL and TL characteristics of quartz sediment grains are preserved during long‐term burial (108 Ma), representing a new tool for interpreting basin evolution and to perform stratigraphic analysis of ancient siliciclastic successions.

Optically stimulated luminescence decay and dosimetric properties of cerium-doped potassium sulfate phosphor.

Optically stimulated luminescence (OSL) is used for dating in archaeology and geology, and in dosimetry of ionizing radiation. Some crystalline wide band-gap insulators may be used as OSL radiation detectors. Recently it was found that cerium-doped potassium sulfate crystals have promising luminescence properties. This paper presents some OSL properties of K2 SO4 :Ce crystals that were prepared in the form of pellets. The crystals exhibited a strong luminescence signal, good measurement repeatability, and high sensitivity for ionizing radiation. Best results were obtained after annealing at 1000°C. Dose-dependence characteristics were determined in the range 10 mGy to 11.2 Gy. OSL decay curves consisted of several components. Fast and slow OSL components of the phosphor had different properties. The slow component was quite stable and obeyed power law dependence. It decayed in the 55 days after irradiation. Its luminescence properties depended on sample preparation and the storage time after irradiation.

Thermoluminescence and optically stimulated luminescence properties of ulexite mineral

Although naturally occurring luminescence materials such as quartz and feldspars are generally used for radiation dosimetry and dating, natural borates may also stand as a promising material for dosimetry and dating. We report thermoluminescence (TL) and optically stimulated luminescence (OSL) of one of the most abundant boron minerals in Turkey namely, ulexite (NaCaB5O6(OH)6·5H2O). An X-ray diffraction (XRD) analysis confirmed that the sample has triclinic crystal structure and contains 40.55% of B, 5.92% of Na2O, 12.3% of CaO. A thermogravimetric analysis indicates two stages of dehydration within 60–160 °C, 160–250 °C and dehydroxylation within 260–580 °C. Analysis of TL glow curves using fractional glow and deconvolution reveal that there are four glow peaks at 154, 211, 273 and 327 °C in the glow curve of ulexite. All the glow peaks follow a non-first order kinetics. The activation energies of the traps are estimated from the fractional glow curves as 0.72, 0.93, 1.16 and 1.28 eV and that evaluated from the deconvolution analysis as 0.76, 0.83, 0.96 and 1.27 eV. The lifetimes of these traps are estimated within 1.55 days–3.6 × 104 years. The radiation dose responses of the TL peaks are supra-linear between 8 Gy and 1024 Gy. OSL decay curve of ulexite consists a fast, a medium and a slow component with recombination lifetimes of (0.63 ± 0.08), (7.51 ± 0.71), (93.49 ± 3.62) s respectively. The fast OSL component obeyed first order, whereas medium and slow components obeyed general order of kinetics. The dose response of the medium and slow OSL components showed a sub-linearity from 64 Gy to 4096 Gy whereas the fast component showed linear response between 8 and 4096 Gy.

Measurement of the paleodose in luminescence dating using the TM-OSL of quartz

The optically stimulated luminescence (OSL) of quartz is widely used in luminescence dating and retrospective dosimetry. The signal exploited up to now in measurement protocol is complex. It is hard to check by standard measurements whether the fast component which is the most appropriate for the age estimation dominates in the total OSL signal. Recently, a new method called thermally modulated OSL (TM-OSL) was developed which allows the selective detection of the OSL components. The new measurement protocol called SAR TM-OSL uses only the fast OSL component to estimate the age. The shape of TM-OSL curve makes possible to distinguish aliquots whose OSL signal is not dominated by the fast OSL component at the first stage of the dating protocol. The new protocol is 30% more time consuming, but it can be easily optimized by stimulation with more powerful LEDs than those used in current experiments.

On the production of the medium component in quartz OSL: Experiments and simulations

Optically stimulated luminescence (OSL) production of the medium component was investigated using a coarse-grained quartz sample from Australia. Analysis of OSL decay curves measured at different stimulation temperatures revealed that there was strong interaction between the initial occupancies of fast and medium OSL components. Preheating experiments showed that the thermal stability of the medium OSL component was almost the same as that of the fast OSL component. These results suggested that both the fast and medium OSL components originate from the same source trap. The production of the medium OSL component was simulated using a kinetic model in which the medium OSL signal was originated from the 325 °C TL trap and the relevant charge is retrapped in the 170 °C TL trap due to the phototransfer effect. A good match between measured and simulated OSL decay curve was achieved.

Optically Stimulated Luminescence Sensitivity of Quartz for Provenance Analysis.

Finding the source or provenance of quartz grains occurring in a specific location allows us to constrain their transport pathway, which is crucial information to solve diverse problems in geosciences and related fields. The optically stimulated luminescence (OSL) sensitivity (light intensity per unit mass per unit radiation dose) has a high capacity for discrimination of quartz sediment grains and represents a promising technique for provenance analysis. In this study, we tested the use of quartz OSL sensitivity (ultraviolet emission) measured under different preheating temperatures and with blue light stimulation at room temperature (~20 °C) for sediment provenance analysis. Quartz OSL sensitivity measured at 20 °C is positively correlated with the sensitivity of an OSL signal measured using procedures (preheat at 190 °C for 10 s, blue stimulation at 125 °C and initial 1 s of light emission) to increase the contribution of the fast OSL component, which has been successfully applied for sediment provenance analysis. The higher OSL signal intensity measured without preheating and with light stimulation at room temperature allows the use of lower given doses, thus reducing measurement time. Additionally, the OSL sensitivity measured at 20 °C in polymineral silt samples of a marine sediment core is also suitable for provenance analysis, as demonstrated by comparison with other independent proxies. OSL signals obtained through light stimulation at room temperature have thus the potential to considerably expand measurement possibilities, including in situ measurements using portable OSL readers.

Luminescence dating of sediments from central Atacama Desert, northern Chile

Abstract This study examines the feasibility of applying luminescence dating methods to quartz and potassium feldspar (K-feldspar) grains from Quaternary continental deposits of the Mejillones Peninsula and Coastal Cordillera in Central Atacama, northern Chile. Sediment burial ages were calculated using single-aliquot regenerative-dose (SAR) protocols applied to the optically stimulated luminescence (OSL) signal of quartz as well as infrared stimulated luminescence (IRSL) and post-infrared infrared stimulated luminescence (post-IR IRSL) signals of K-feldspar. Considering that the target sedimentary deposits comprise the Late Pleistocene age range, K-feldspar grains were dated using fading-corrected IRSL signals measured at 50 °C (IR50) and post-IR IRSL measured at 225 °C (pIRIR225) to minimize the potential effect of residual doses on calculated ages. The results of the analytical procedures indicate that quartz grains extracted from the studied sediments present a very weak or even no fast OSL component. The combination of a low OSL sensitivity, signal instability and equivalent dose distributions with high overdispersion (>40% for most samples) hinder reliable age estimation using quartz aliquots. Bleaching test results show that the IR50 signal from K-feldspar aliquots is well reset after 20–24 h of light exposure, while the pIRIR225 signal may present residual doses corresponding to between 10 and 15% of the natural signal. IR50 fading rates are ∼6–7%/decade for most studied samples, with exception of one sample which yielded a g-value of 18.77 ± 2.06%/decade. Fading rates for the pIRIR225 signal yielded variable results among sampling sites, with g-values ranging between 0.70 ± 0.24 and 6.77 ± 1.05%/decade. The dating results point out that quartz OSL ages are largely underestimated in relation to K-feldspar fading-corrected IR50 and pIRIR225 ages. Fading-corrected pIRIR225 K-feldspar ages indicate that the alluvial sedimentation in the downthrown block of an active normal fault in Mejillones Peninsula occurred between 163.4 ± 18.4 ka and 87.4 ± 6.6 ka. K-feldspar ages also allow to constrain the age of fault scarp degradation and fault reactivation in two main branches of the Atacama Fault System. In the Naguayan Fault, pIRIR225 ages indicate that faulting occurred after 21.4 ± 3.2 ka while in the Salar del Carmen Fault, faulting is recorded after 14.7 ± 1.0 ka.

Thermally modulated OSL related to the fast component of the OSL signal in quartz

The methods of optically stimulated luminescence (OSL) measurements used until recently applied optical stimulation at a constant temperature, with a constant stimulation energy and a constant or linearly increased flux of stimulation photons. During such stimulation the optical cross-section of traps is invariable and it is hard to separate the signals of different origins. It was shown recently that the selective optical emptying of traps is much easier when the optical cross-section is changed during the stimulation. Due to the dependence of the optical cross-section on temperature advantageous changes in this trap parameter can be induced by increasing the sample temperature during optical stimulation. Such a method can be called thermally modulated OSL (TM-OSL). When the experimental conditions are properly selected the TM-OSL curve has the form of a peak. The shape and position of this peak are uniquely determined by the trap parameters and, therefore, curve analysis can be used to estimate the optical depth of the trap (photoionization threshold) and the strength of electron-lattice coupling. These parameters define traps unambiguously and allow a direct correlation of the traps active in the OSL and TL processes to be made. The position of the TM-OSL peak on the temperature axis depends greatly on the stimulation energy, the heating rate and the photon flux used for optical stimulation, so these experimental factors can be used to separate the individual OSL components. This work focuses on the selective detection of the fast component of the quartz OSL signal. The traps responsible for the fast OSL component can be depopulated by light with the wavelength of 620 nm, which is far longer the usual 470 or 530 nm used in OSL measurements of quartz. The results of such experiments, when supported by computer simulations of the thermally modulated OSL process, allow the value of 3 eV to be estimated for the optical depth of traps responsible for the fast OSL component in quartz.

BeO optically stimulated luminescence dosimetry using automated research readers

The objective of this work is to develop a methodology for precise optically stimulated luminescence (OSL) dosimetry using BeO chips and an automated research reader (Risø TL/OSL reader, Risø National Laboratory), documenting optimum detector preparation procedures, readout conditions, sensitivity, minimum detectable dose, and precision. We investigated the influence of stimulation wavelengths (green versus blue LEDs), pre-irradiation annealing conditions, reproducibility, sensitivity changes with dose or annealing, and precisions in the dose response curve with a reference irradiation. The results demonstrate that with proper annealing (700 °C/15 min) and the readout procedure described here (blue stimulation, total OSL area as the signal, and a fixed dose to correct for detector sensitivity, among other factors), a precision <1% (experimental standard deviation of the data) can be obtained with BeO. A fast OSL component that decays within 0.5 s was observed, but does not affect the results significantly except in specific conditions (initial intensity as the OSL signal, readout within 10 min following irradiation). Sensitivity changes were observed as a function of both readout time and dose, pointing out the need for annealing to reset the sensitivity. Other practical aspects, such as the cross-irradiation and bleaching in the automated reader, and the sensitivity of the signal to dim room red light were also tested. This work provides the basis and a demonstration of a protocol for new users interested in employing BeO for different dosimetry applications, including in medicine, using automated research OSL readers.

Quartz OSL dating of late Holocene beach ridges from the Magdalen Islands (Quebec, Canada)

Quartz optically stimulated luminescence (OSL) dating has been applied to sandy beach ridge systems from the Magdalen Islands in the center of the Gulf of St. Lawrence (Quebec, Canada) to provide the first chronological framework for these features. Nineteen beach ridges (22 samples) from four different sites throughout the archipelago were investigated. At one of the sites, samples were taken at 9 m and 7.5 m depth using a vibracore. The quartz is dominated by the fast OSL component and a single-aliquot regenerative-dose (SAR) protocol was used to measure the equivalent doses; a low preheat (180°C/10 s) was chosen to avoid the influence of thermal transfer. The average dose recovery ratio of all samples is 1.02 ± 0.02 (n = 130) suggesting that the SAR protocol works satisfactorily on this material. The OSL ages are internally consistent and supported by independent age control (radiocarbon). The OSL ages indicate that the ridges were built between 2.6 ± 0.2 ka and 0.40 ± 0.10 ka, i.e. during a period of sea level rise. This rise eroded adjacent sandstone cliffs, which contributed a significant sediment supply to the littoral drift and beaches. Some low-lying coasts in the archipelago are still prograding, despite a relative sea level increase of ∼1.6 mm/a over the last 600 years. The late Holocene ages obtained in this study indicate that these processes have been active for at least the past two thousand years. This study demonstrates for the first time that OSL dating using quartz has great potential in this area, and is an appropriate method for establishing precise chronologies for coastal sediments in this region of the Gulf of St. Lawrence.

The origin of the medium OSL component in West Australian quartz

Optically stimulated luminescence (OSL) of a coarse-grained sedimentary quartz from West Australia was investigated. Observations of OSL and TL (thermoluminescence) were made following a series of experiments using different heating and optical bleaching conditions, and with optical stimulation at several different temperatures. Analysis of the fast and medium OSL components suggests that the medium OSL component observed after heating at 260°C is a by-product of the production of the fast component, and both of them have as their original source the 325°C TL trap. During fast OSL production following irradiation and preheating, some of the electrons evicted into the conduction band are re-trapped in an intermediate trap corresponding to the 170°C TL peak; from here they are instantaneously stimulated to give rise to the medium OSL signal when the blue light stimulation is switched on, and subsequently result in the residual recuperated TL after the blue light is switched off. The kinetic properties of the medium OSL component are determined by the properties of both the 170°C and 325°C TL traps in contrast to the conventional interpretation of the medium component being derived from an independent source trap. Therefore, the 170°C TL trap also plays unexpected roles in quartz OSL production with elevated stimulation temperatures (e.g. 125°C or 130°C, currently used for OSL dating), while the 110°C TL trap and its influences are being avoided.

Variations in quartz OSL components with lithology, weathering and transportation

The signal properties of quartz optically stimulated luminescence (OSL) vary from sample to sample, and even from grain to grain, in terms of, for example, signal intensity or the composition of OSL signal components. However, the cause of the variation in quartz OSL properties is not well understood. Here, we report our experimental observations of continuous wave and linearly modulated OSL signals in quartz grains from fresh bedrocks, saprolites, and sediments in Korea. The OSL signals in quartz grains from both fresh bedrocks and saprolites in the granitic and metamorphic rocks are dominated by slower OSL components, with no fast OSL component. By contrast, the OSL signals in quartz extracts from sandstones are predominantly composed of fast OSL components. Quartz extracts derived from thermally metamorphosed or diagenetically recrystallised sandstones, however, tend to emit weaker OSL signals, a property related to intense slower OSL components. Along the fluvial transportation path, slower OSL components dominate near the host granite, but their absolute/relative intensity decreases with a simultaneous increase in the fast OSL component with transportation distance. OSL signal characteristics suitable for dating appear to be acquired during sedimentary processes after the liberation of quartz grains from granitic and metamorphic bedrock. Therefore, granitic and metamorphic quartz grains should be transported a sufficient distance for the fast OSL component to be sensitised. However, unless they have been affected by post-thermal metamorphism and recrystallisation, the OSL signal properties of quartz grains released from Cretaceous sedimentary rocks seem to be suitable for OSL dating, regardless of the transportation distance.

How to visualize quartz OSL signal components

The optically stimulated luminescence (OSL) signal of natural quartz measured under constant stimulation power (CW-OSL) is a featureless decay curve where underlying components cannot be identified easily. Visual interpretation of quartz OSL signals is easier if signals are shown in spectrum-like form. This can be achieved either through ramped stimulation, or by transforming a measured CW-OSL curve into a pseudo OSL curve. We show that both give similar results, but that transformation should be preferred as CW-OSL provides best signal-to-noise ratios. We present different transformation methods to obtain pseudo OSL curves and discuss the advantages and disadvantages of each method. In addition, we show that different pseudo OSL transformations can be used to emphasize specific aspects of the OSL signal. We conclude that transformation of CW-OSL to pseudo hyperbolically modulated OSL provides the most useful visualization of the quartz fast OSL component. Pseudo parabolic modulated OSL is the transformation of choice for showing the slow component(s). The pseudo OSL curves can be used for rapid visual inspection of the relative contribution of the OSL components prior to further analysis.

Thermal history versus sedimentary history: OSL sensitivity of quartz grains extracted from rocks and sediments

The optically stimulated luminescence (OSL) sensitivity of quartz has a significant influence on luminescence dating procedures. Furthermore, identifying the natural controls of quartz OSL sensitivity is an important step towards new applications of OSL in geology such as provenance tracing. We evaluate the OSL sensitivity (total and the proportion of the informally assigned fast, medium and slow components) of single grains of quartz extracted from 10 different igneous and metamorphic rocks with known formation conditions; and from fluvial and coastal sediments with different sedimentary histories and known source rocks. This sample suite allows assessment of the variability of the OSL sensitivity of single quartz grains with respect to their primary origin and sedimentary history. We observed significant variability in the OSL sensitivity of grains within all studied rock and sediment samples, with the brightest grains of each sample being those dominated by the fast component. Quartz from rocks formed under high temperature (>500 °C) conditions, such as rhyolites and metamorphic rocks from the amphibolite facies, display higher OSL sensitivity. The OSL sensitivity of fluvial sediments which have experienced only a short transport distance is relatively low. These sediments show a small increase in OSL sensitivity downstream, mainly due to a decreasing fraction of “dim” grains. The quartz grains from coastal sands present very high sensitivity and variability, which is consistent with their long sedimentary history. The high variability of the OSL sensitivity of quartz from coastal sands is attributed more to the mixture of grains with distinct sedimentary histories than to the provenance from many types of source rocks. The temperature of crystallization and the number of cycles of burial and solar exposure are suggested as the main natural factors controlling the OSL sensitivity of quartz grains. The increase in OSL sensitivity due to cycles of erosion and deposition surpasses the sensitivity inherited from the source rock, with this increase being mainly related to the sensitization of fast OSL components. The discrimination of grains with different sedimentary histories through their OSL sensitivities can allow the development of quantitative provenance methods based on quartz.

Selection of integration time intervals for quartz OSL decay curves

In quartz optically stimulated luminescence (OSL) dating protocols, an initial integral of the OSL decay curve is used in the calculation of equivalent dose, once a background integral has been subtracted. Because the OSL signal commonly contains a number of exponentially decaying components, the exact choice of time intervals used for the initial-signal and background integrals determines the composition of the net signal. Here we investigate which combination of time intervals will produce the net signal most dominated by the fast OSL component, while keeping an acceptable level of precision. Using a three-component model of OSL decay, we show that for a specified level of precision, the net signal most dominated by the fast component can be obtained when the background integral immediately follows the initial signal and is approximately 2.5 times its length. With this ‘early-background’ approach, the contribution of slow components to the net signal is virtually zero. We apply our methods to four samples from relatively young deposits. Compared to the widely used ‘late-background’ approach, in which the background integral is taken from the last few seconds of OSL, we find less thermal transfer, less recuperation and a higher proportion of aliquots yielding an equivalent dose in agreement with expectations. We find the use of an early background to be a simple and effective way of improving the accuracy of OSL dating, and suggest is should be used in standard protocols.

Investigating age underestimation in the high dose region of optically stimulated luminescence using fine grain quartz

The age range of the single-aliquot regenerative-dose (SAR) protocol applied to quartz optically stimulated luminescence (OSL) has become the subject of debate as age underestimations for samples of Eemian age (ca. 125 ka) and older are increasingly reported. In order to investigate the origin of the age underestimation, the behaviour of fine grain quartz samples taken from two sites was compared. Sediment from both sites originates in the Alps, with those from Azzano Decimo, northeastern Italy, already displaying a significant age underestimation before reaching the Eemian, while ages for samples from Niederweningen, northern Switzerland, agree with expected ages well beyond the Eemian. Estimated dose (D e) values for both sets of samples are up to around 400 Gy, and all meet the usual performance criteria for testing the reliability of the SAR protocol. D e values determined using a sensitivity-corrected multiple aliquot regenerative-dose (MAR) protocol were within 10% of those determined using a SAR protocol for both sites, and so could not overcome the significant underestimation seen at Azzano Decimo. Lifetime calculations confirmed the stability of the signal well beyond the age range required at both sites, for both the initial integral as well as that used for an early background subtraction. The relative percentage contribution of the fast and medium OSL components to the initial integral remained constant in both the natural signal and similar sized laboratory generated doses. The quartz OSL from both sites displayed similar characteristics under all analyses and no indication was found for the possible origin of the age underestimation seen at Azzano Decimo. In the comparisons made between the dose–response of both laboratory and naturally generated signals in these samples, no evidence was found to suggest that the presence of the high dose linear region is restricted to the laboratory. The reliability of quartz OSL ages derived from this part of the curve however, remain in question, and require the support of independent age control until a performance criterion can be found with which to test it.

Investigating quartz optically stimulated luminescence dose–response curves at high doses

Despite the general expectation that optically stimulated luminescence (OSL) growth should be described by a simple saturating exponential function, an additional high dose component is often reported in the dose response of quartz. Although often reported as linear, it appears that this response is the early expression of a second saturating exponential. While some studies using equivalent doses that fall in this high dose region have produced ages that correlate well with independent dating, others report that it results in unreliable age determinations. Two fine grain sedimentary quartz samples that display such a response were used to investigate the origin of this additional high dose component: three experiments were conducted to examine their dose–response up to >1000 Gy. The high dose rates provided by laboratory irradiation were found not to induce a sensitivity change in the response to a subsequent test dose, with the latter not being significantly different from those generated following naturally acquired doses. The relative percentage contributions of the fast and medium OSL components remained fixed throughout the dose–response curve, suggesting that the electron traps that give rise to the initial OSL do not change with dose. An attempt was made to investigate a change in luminescence centre recombination probability by monitoring the depletion of the ‘325 °C’ thermoluminescence (TL) during the optical stimulation that would result in depletion of the OSL signal. The emissions measured through both the conventional ultraviolet (UV), and a longer wavelength violet/blue (VB) window, displayed similar relative growth with dose, although it was not possible to resolve the origin of the VB emissions. No evidence was found to indicate whether the additional component at high doses occurs naturally or is a product of laboratory treatment. However, it appears that these samples display an increased sensitivity of quartz OSL to high doses that is not recorded by the sensitivity to a subsequent test dose, and which results in a change in the sensitivity-corrected dose–response curve.